EP0635716A1 - Asymmetrischer 4-Kristallmonochromator - Google Patents

Asymmetrischer 4-Kristallmonochromator Download PDF

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Publication number
EP0635716A1
EP0635716A1 EP94202026A EP94202026A EP0635716A1 EP 0635716 A1 EP0635716 A1 EP 0635716A1 EP 94202026 A EP94202026 A EP 94202026A EP 94202026 A EP94202026 A EP 94202026A EP 0635716 A1 EP0635716 A1 EP 0635716A1
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EP
European Patent Office
Prior art keywords
crystal
monochromator
ray
crystals
end faces
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP94202026A
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English (en)
French (fr)
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EP0635716B1 (de
Inventor
Paul C/O Int.Octrooibureau B.V. Van Der Sluis
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Koninklijke Philips NV
Original Assignee
Koninklijke Philips Electronics NV
Philips Electronics NV
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Publication date
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Publication of EP0635716A1 publication Critical patent/EP0635716A1/de
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    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—HANDLING OF PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K1/00—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating
    • G21K1/06—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating using diffraction, refraction or reflection, e.g. monochromators
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—HANDLING OF PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K2201/00—Arrangements for handling radiation or particles
    • G21K2201/06—Arrangements for handling radiation or particles using diffractive, refractive or reflecting elements
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—HANDLING OF PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K2201/00—Arrangements for handling radiation or particles
    • G21K2201/06—Arrangements for handling radiation or particles using diffractive, refractive or reflecting elements
    • G21K2201/062—Arrangements for handling radiation or particles using diffractive, refractive or reflecting elements the element being a crystal

Definitions

  • the invention relates to an X-ray analysis apparatus, comprising an X-ray source, a wavelength-dispersive system of crystals, an object carrier, and an X-ray detection system.
  • the invention also relates to a crystal monochromator and to a crystal analyser for such an apparatus.
  • An X-ray analysis apparatus of this kind is known from US 4,567,605. So as to achieve notably a high resolution, the apparatus described therein comprises a dispersive element in the form of a 4-crystal monochromator. For specific applications, for example examination of thin layers, be it imperfect as well as epitaxial layers and the like, the comparatively low radiation intensity of the known 4-crystal monochromators may become objectionable. Increasing the radiation intensity by using a high-intensity radiation source makes the apparatus expensive and substantially limits the service life of the radiation source.
  • the X-ray analysis apparatus of the kind set forth in accordance with the invention is characterized in that reflective crystal end faces of a dispersive crystal do not extend parallel to diffractive crystal lattice planes in the crystals.
  • the crystal end faces in the monochromator in accordance with the invention do not extend parallel to the crystal lattice planes in the crystals, a larger acceptance angle is realised for an X-ray beam to be monochromatized.
  • the phenomenon that the crystal end faces used do not extend parallel to the crystal lattice planes is referred to as asymmetry in the context of the present invention.
  • the high resolution of the known 4-crystal monochromator can be sacrificed for a high intensity then required.
  • the use of the monochromator in accordance with the invention enables faster analysis with a better signal-to-noise ratio.
  • reflecting crystal end faces form part of a 4-crystal monochromator.
  • such a monochromator undergoes hardly any or no exterior geometrical modifications relative to the known monochromator, so that it can be included in an X-ray analysis apparatus without requiring complex adaptations.
  • the four crystal end faces preferably enclose the same angle with respect to the relevant crystal lattice planes, but for specific applications deviations therefrom are feasible.
  • the crystals consist of, for example monocrystalline germanium, the diffractive crystal lattice planes being formed by (220) or (440) lattice planes. Because the (220) lattice planes already produce a higher intensity, it is advantageous to use an asymmetrical monochromator in accordance with the invention in the (220) position.
  • the angle between the crystal end faces and the crystal lattice planes amounts to, for example from approximately 150 to 23° for the (220) position.
  • Such a monochromator produces a effective X-ray beam having an intensity which is approximately x times higher than that of the known symmetrical monochromator.
  • x 4 for 15°.
  • the (440) crystal plane mode still acts as the high resolution mode.
  • x 15 for 20.6°.
  • the angle is chosen so that the crystal end faces, measured in the diffraction direction, are large enough to accept the entire incident beam.
  • the value of the angle can also adapted to a desired effective beam intensity for specific examinations.
  • the monochromator carrier may be constructed so that different measurement modes can be selected by rotation of the crystal pairs, for example an asymmetrical (220) position for high intensity and a (440) position for high resolution.
  • different measurement modes can be selected by rotation of the crystal pairs, for example an asymmetrical (220) position for high intensity and a (440) position for high resolution.
  • a range of zero intensity is traversed during rotation of the crystal pairs.
  • no reflection will occur any more for any angular rotation. Alignment of the experimental arrangement then becomes very difficult.
  • the monochromator holder is constructed as a changer system whereby several monochromators can be alternately positioned in the beam path. Because rotation of the crystal pairs is thus avoided, the alignment problem no longer occurs.
  • a monochromator carrier in the form of a changer may also comprise asymmetrical crystals as well as symmetrical crystals with a (220) position as well as a (440) position for the crystals, so that crystal rotation is no longer necessary.
  • An X-ray monochromator suitable for an X-ray analysis apparatus in accordance with the invention is provided with crystals whose crystal end faces do not extend parallel to diffractive crystal lattice planes.
  • Different crystal lattice planes can be chosen for this purpose; however, crystal lattice planes which already produce a comparatively high effective beam in a symmetrically ground crystal (i.e . a crystal in which the crystal end face extends parallel to the relevant crystal lattice planes), are most suitable for this purpose.
  • Fig. 1 shows an X-ray analysis apparatus with an X-ray source 1, a monochromator 3, a goniometer 5 and a detector 7 which are only diagrammatically shown.
  • the X-ray source 1 comprises an anode 14 which is accommodated in a housing 10 provided with a radiation window 12, which anode consists of, for example copper, chromium, scandium or another customary anode material.
  • An electron beam generates an X-ray beam 15 in the anode.
  • the monochromator comprises two crystal pairs 18 and 20 with crystals 21, 23, 25 and 27.
  • crystal pair 18 crystal end faces 22 and 24 serve as active crystal faces.
  • crystal pair 20 crystal end faces 26 and 28 act as active crystal faces.
  • the first crystal pair can be arranged so as to be rotatable about an axis 30 extending perpendicularly to the plane of drawing, and the second crystal pair can be arranged similarly so as to be rotatable about an axis 32.
  • the end faces 22, 24 and 26, 28 remain mutually parallel in any rotary position.
  • the crystals have, for each pair, a U-shape cut from a single monocrystal, the connecting portion of the U being used, for example for mounting the crystals.
  • the inner faces of the limbs of the U then form the active crystal end faces. After cutting and possibly grinding or polishing, a surface layer has been removed from these surfaces, for example by etching, in order to remove material in which stresses may have developed due to mechanical working.
  • the carrier plate 34 for the monochromator has a comparatively rigid construction so that, for example its lower side can be used to support mechanical components, for example for the crystal orientation motions, without risking deformation of the plate.
  • the length of one of the crystals of each of the crystal pairs is reduced so that more freedom is obtained in respect of a beam path.
  • the attractive property of the 4-crystal monochromator as regards the angle of aperture for the incoming beam enables the X-ray source, i.e . actually a target spot on the anode 14, to be situated at a minimum distance from the first crystal pair, which minimum distance is determined by the construction of the source. An attractive intensity is thus achieved already for the ultimate analysing X-ray beam 35.
  • the first crystal pair 18 is rotatable about the axis 30 of a shaft on which a first friction wheel 40 which is situated beneath the mounting plate is mounted so as to engage a second friction wheel 42 which is mounted on the shaft with the axis 32 about which the second crystal pair 20 is rotatable.
  • the two crystal pairs may alternatively be mutually independently adjustable or the adjustment can be performed by means of a drive motor with, for example programmed settings adapted to the anode material to be used or to specimens to be analysed.
  • the crystals are preferably made of germanium having active end faces which extend parallel to the (440) crystal faces of a germanium monocrystal which is relatively free from dislocations.
  • an extremely well monochromatized beam having, for example a relative wavelength width of 2.3 x 10 ⁇ 5, a divergence of, for example 5 arc seconds, and an intensity of up to, for example 3 x 104 quants per second per cm2 can be formed.
  • Such a sharply defined beam enables measurement of errors in lattice spacings of up to 1 to 105 can be measured and high-precision absolute crystal lattice measurements can also be performed thereby.
  • the monochromatization of the X-ray beam is realized in the monochromator by the central two reflections, i.e . the reflections from the crystal faces 24 and 28.
  • the two reflections from the end faces 22 and 26 do influence the beam parameters, but they guide the beam 35 in the desired direction coincident with the prolongation of the incoming beam 15. Wavelength adjustment is achieved by rotating the two crystal pairs in mutually opposite directions; during this motion, therefore, the position of the emergent beam 35 does not change.
  • An intensity which is, for example 30 times higher can be achieved by utilizing reflections from (220) crystal faces, in which case a larger spread in wavelength and a larger divergence occur.
  • the monochromator is non-rotatably connected to the goniometer 5 in which a specimen 46 to be analysed is accommodated in a specimen holder 44.
  • a detector 7 which is rotatable along a goniometer circle 48 in known manner. The detector enables measurements to be made throughout a larger angular range and for different orientations of the specimen.
  • the goniometer may include an optical encoder which is not shown in the drawing.
  • Fig. 2b shows an example of an asymmetrical system of crystals in accordance with the invention, compared with a similar symmetrical system as shown in Fig. 2a, comprising notably germanium crystals with (440) and (220) lattice planes, respectively.
  • Fig. 2a shows the symmetrical system comprising crystals 21, 23, 25 and 27 in which the lattice planes extend parallel to crystal end faces 22, 24, 26 and 28, respectively.
  • each crystal exhibits (220) as well as (440) lattice planes; in the upper crystal pairs of the Figs. 2a and 2b the (440) lattice planes are used, whereas in the lower crystal pairs of the Figs. 2a and 2b the (220) lattice planes are used.
  • An incoming X-ray beam 15 emerges from the crystal system as a beam 35 which is collinear with the incident beam in all situations.
  • a comparison of the beam diameter of the Figs. 2a and 2b already demonstrates that the difference between the symmetrical and the non-symmetrical system is comparatively small for the (440) crystal planes, whereas it is substantial for the (220) crystal planes. The same holds for the resolution.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
EP94202026A 1993-07-19 1994-07-13 Asymmetrischer 4-Kristallmonochromator Expired - Lifetime EP0635716B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
BE9300753 1993-07-19
BE9300753A BE1007349A3 (nl) 1993-07-19 1993-07-19 Asymmetrische 4-kristalmonochromator.

Publications (2)

Publication Number Publication Date
EP0635716A1 true EP0635716A1 (de) 1995-01-25
EP0635716B1 EP0635716B1 (de) 2002-01-09

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Family Applications (1)

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EP94202026A Expired - Lifetime EP0635716B1 (de) 1993-07-19 1994-07-13 Asymmetrischer 4-Kristallmonochromator

Country Status (5)

Country Link
US (1) US5509043A (de)
EP (1) EP0635716B1 (de)
JP (1) JP3706641B2 (de)
BE (1) BE1007349A3 (de)
DE (1) DE69429598T2 (de)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996037898A1 (en) * 1995-05-23 1996-11-28 Korytar Dusan The equipment for x-ray beam conditioning
FR2754102A1 (fr) * 1996-09-27 1998-04-03 Nec Corp Procede de generation d'un microfaisceau de rayons x et dispositif pour celui-ci

Families Citing this family (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6041098A (en) * 1997-02-03 2000-03-21 Touryanski; Alexander G. X-ray reflectometer
US6332017B1 (en) 1999-01-25 2001-12-18 Vanderbilt University System and method for producing pulsed monochromatic X-rays
US6327335B1 (en) 1999-04-13 2001-12-04 Vanderbilt University Apparatus and method for three-dimensional imaging using a stationary monochromatic x-ray beam
JP4313844B2 (ja) * 2000-05-31 2009-08-12 株式会社リガク チャンネルカットモノクロメータ
JP4498663B2 (ja) * 2001-07-11 2010-07-07 学校法人東京理科大学 透過型結晶分析体の厚さ設定方法
AU2003298591A1 (en) * 2002-09-23 2004-05-04 Johns Hopkins University Double crystal analyzer linkage
US7486984B2 (en) * 2004-05-19 2009-02-03 Mxisystems, Inc. System and method for monochromatic x-ray beam therapy
DE102004027347B4 (de) * 2004-05-27 2008-12-24 Qimonda Ag Wellenlängenselektor für den weichen Röntgen- und den extremen Ultraviolettbereich
FI20041538L (fi) * 2004-11-29 2006-05-30 Stresstech Oy Goniometri
JP4679975B2 (ja) * 2005-06-15 2011-05-11 財団法人電力中央研究所 単結晶試料における面内配向した転位線を有する結晶欠陥のｘ線トポグラフによる撮影方法
JP4773899B2 (ja) * 2006-06-29 2011-09-14 株式会社リガク Ｘ線分光測定方法およびｘ線分光装置
US8537967B2 (en) * 2009-09-10 2013-09-17 University Of Washington Short working distance spectrometer and associated devices, systems, and methods
US20130108023A1 (en) * 2011-11-02 2013-05-02 Alex Deyhim Development of a double crystal monochromator
KR20130087843A (ko) * 2012-01-30 2013-08-07 한국전자통신연구원 단결정 물질을 이용한 엑스선 제어 장치
US9269468B2 (en) * 2012-04-30 2016-02-23 Jordan Valley Semiconductors Ltd. X-ray beam conditioning
US9966161B2 (en) * 2015-09-21 2018-05-08 Uchicago Argonne, Llc Mechanical design of thin-film diamond crystal mounting apparatus with optimized thermal contact and crystal strain for coherence preservation x-ray optics
DE102015226101A1 (de) * 2015-12-18 2017-06-22 Bruker Axs Gmbh Röntgenoptik-Baugruppe mit Umschaltsystem für drei Strahlpfade und zugehöriges Röntgendiffraktometer
WO2017117197A1 (en) * 2015-12-28 2017-07-06 University Of Washington Methods for aligning a spectrometer
JP2019191168A (ja) 2018-04-23 2019-10-31 ブルカー ジェイヴィ イスラエル リミテッドＢｒｕｋｅｒ Ｊｖ Ｉｓｒａｅｌ Ｌｔｄ． 小角ｘ線散乱測定用のｘ線源光学系
CN112654861B (zh) 2018-07-05 2024-06-11 布鲁克科技公司 小角度x射线散射测量
US11576636B2 (en) * 2019-05-10 2023-02-14 Illinois Institute Of Technology Apparatus and method for analyzer-based contrast imaging with a polychromatic beam
US11781999B2 (en) 2021-09-05 2023-10-10 Bruker Technologies Ltd. Spot-size control in reflection-based and scatterometry-based X-ray metrology systems
US12249059B2 (en) 2022-03-31 2025-03-11 Bruker Technologies Ltd. Navigation accuracy using camera coupled with detector assembly

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EP0110469A2 (de) * 1982-11-25 1984-06-13 Koninklijke Philips Electronics N.V. Apparat zur Röntgenstrahlenanalyse, mit einem Vierkristallmonochromator
US4928294A (en) * 1989-03-24 1990-05-22 U.S. Government As Represented By The Director, National Security Agency Method and apparatus for line-modified asymmetric crystal topography

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US4821301A (en) * 1986-02-28 1989-04-11 Duke University X-ray reflection method and apparatus for chemical analysis of thin surface layers
US5287395A (en) * 1992-07-06 1994-02-15 The United States Of America As Represented By The United States Department Of Energy Inclined monochromator for high heat-load synchrotron x-ray radiation

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EP0110469A2 (de) * 1982-11-25 1984-06-13 Koninklijke Philips Electronics N.V. Apparat zur Röntgenstrahlenanalyse, mit einem Vierkristallmonochromator
US4928294A (en) * 1989-03-24 1990-05-22 U.S. Government As Represented By The Director, National Security Agency Method and apparatus for line-modified asymmetric crystal topography

Non-Patent Citations (3)

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H.HASHIZUME ET AL.: "DYNAMICAL X-RAY DIFFRACTION FROM A PERFECT CRYSTAL UNDER GRAZING INCIDENCE CONDITIONS", REVIEW OF SCIENTIFIC INSTRUMENTS, vol. 60, no. 7, July 1989 (1989-07-01), NEW YORK US, pages 2373 - 2375, XP000038372, DOI: doi:10.1063/1.1140723 *
K.KOHRA ET AL.: "DESIGN OF HIGH RESOLUTION X-RAY OPTICAL SYSTEM USING DYNAMICAL DIFFRACTION FOR SYNCHROTRON RADIATION", NUCLEAR INSTRUMENTS AND METHODS, vol. 152, 1978, AMSTERDAM NL, pages 161 - 166 *
MASAO KURIYAMA: "MATERIALS SCIENCE WITH SR USING X-RAY IMAGING SPATIAL RESOLUTION/SOURCE SIZE", NUCLEAR INSTRUMENTS AND METHODS RESEARCH A, vol. A303, no. 3, 15 June 1991 (1991-06-15), AMSTERDAM NL, pages 503 - 514, XP000234162 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996037898A1 (en) * 1995-05-23 1996-11-28 Korytar Dusan The equipment for x-ray beam conditioning
FR2754102A1 (fr) * 1996-09-27 1998-04-03 Nec Corp Procede de generation d'un microfaisceau de rayons x et dispositif pour celui-ci
NL1007118C2 (nl) * 1996-09-27 1998-05-08 Nec Corp Werkwijze voor het opwekken van een röntgenstralenmicrobundel en inrchting daarvoor.
FR2756449A1 (fr) * 1996-09-27 1998-05-29 Nec Corp Procede de generation d'un microfaisceau de rayons x et dispositif pour celui-ci
US5914998A (en) * 1996-09-27 1999-06-22 Nec Corporation X-ray microbeam generating method and device for the same

Also Published As

Publication number Publication date
DE69429598T2 (de) 2002-08-29
BE1007349A3 (nl) 1995-05-23
JP3706641B2 (ja) 2005-10-12
EP0635716B1 (de) 2002-01-09
JPH0755729A (ja) 1995-03-03
US5509043A (en) 1996-04-16
DE69429598D1 (de) 2002-02-14

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